反应 #586124

ord-0fbc315e828d4f1596636d7f04b90a6e

反应方程式

O
water
Cc1ccc(-c2c(Cl)cc(C(F)(F)F)cc2Cl)cc1Sc1cc(-c2c(Cl)cc(C(F)(F)F)cc2Cl)ccc1C
1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene]
O=S([O-])CO.[Na+]
Rongalite
CC(C)I
isopropyl iodide
Cc1ccc(-c2c(Cl)cc(C(F)(F)F)cc2Cl)cc1SC(C)C
[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylphenyl] isopropyl sulfide
收率 75.3%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The resulting reaction mixture
  2. 2
    萃取extracted with 50 ml of ethyl acetate twice
  3. 3
    洗涤The ethyl acetate layer was washed with 50 ml of water twice
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
  6. 6
    其他Purification of the residue by silica gel column chromatography

实验过程

3.3 g (4.9 mmol) of 1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene], 3.0 g (19.5 mmol) of Rongalite and 3.0 g (17.6 mmol) of isopropyl iodide were stirred in 30 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.4 g of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylphenyl] isopropyl sulfide (yield 38.0%) as a yellow dough (nD20 1.5462).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767626B2uspto-grants-2010_08